Method for producing a metal alloy strip

ABSTRACT

A method for producing a metallic strip is disclosed. A metallic melt containing above about 20% by weight of iron is formed into a strip so that fine iron particles are distributed throughout. The strip may be rolled to elongate the iron particles.

This application is a continuation-in-part of U.S. Ser. No. 499,008,filed May 27, 1983, (now abandoned).

This application relates to U.S. Pat. No. 4,544,463 entitled Method ForProducing Acicular Or Equiaxed Iron Or Iron Alloy Particles, by MichaelJ. Pryor; U.S. Pat. No. 4,540,477 entitled Apparatus For ProducingAcicular Or Equiaxed Iron or Iron Alloy Particles, by Lifun Lin; U.S.patent application Ser. No. 773,769 entitled Chemical Process ForExtracting Fe Particles From Cu-Fe Strips, by Lifun Lin, filed Sept. 9,1985; and U.S. patent application Ser. No. 803,379 entitled Method OfProducing Ferromagnetic Particles, by Jacob Crane et al., filed Dec. 2,1985.

While the invention is subject to a wide range of applications, itespecially relates to the formation of a thin continuous metallic striphaving equiaxed or oriented ferromagnetic particles distributedthroughout. More particularly, the metallic strips are suitable for amagnetic tape medium or as an intermediate material for making iron oriron alloy particles.

In the past, improvements in magnetic tape performance were largelyfocused in two areas. Firstly, improvements in the remanence andcoercivity of the magnetic particles were achieved by factors such asdoping and optimizing particle size, morphology and purity. Secondly,improved distribution and alignment of particles which improve theremanent induction and coercivity were achieved by various processcontrols. However, performance limitations remain due to agglomerationof ferromagnetic particles and a lack of particle orientation in thelongitudinal direction.

Thin ribbons of magnetic material have been manufactured using a chillsurface similar to that described in the present invention. For example,U.S. Pat. No. 4,257,830 to Tsuya et al. discloses "a thin ribbon ofmagnetic material having a high permeability, excellent flexibility andworkability, and consisting essentially of by weight 4-7% of aluminum,8-11% of silicon and the remainder substantially iron and inevitableimpurities and having a compact fine grain crystalline structure withoutexisting substantially an ordered lattice." Although the disclosed thinstrip forming technique includes steps similar to that of the presentinvention, the formed material is completely different. U.S. Pat. Nos.4,330,027 and 4,221,257 also disclose the method of making continuousmetallic amorphous strips using a chill body.

Magnetizable tape of a thin sheet of highly magnetizable alloy andprovided with a thin backing of high tensile, flexible, substantiallynon-stretchable material is disclosed in U.S. Pat. No. 3,186,707.However, this patent does not suggest or teach forming a metallic stripsimilar to that of the present invention.

In particular, the present invention relates to a magnetizable stripwhich is primarily fabricated from iron and a matrix of metal or metalalloy. There is considerable art describing the melting and casting ofhigh compositions of iron and a metal or alloy such as copper disclosedin U.S. Pat. Nos. 2,754,193, 2,754,194 and 3,583,864. However, none ofthese patents suggest processing the copper-iron mixture to provide themagnetic properties inherent in the present invention.

It is a problem underlying the present invention to provide a method forproducing a metallic strip having equiaxed or accicular ferromagneticparticles which are not agglomerated and which may be homogeneouslydistributed throughout the strip.

It is an advantage of the present invention to provide a method forproducing a metal or alloy strip which obviates one or more of thelimitations and disadvantages of the described prior arrangements.

It is a further advantage of the present invention to provide a methodfor producing a metal or alloy strip having homogeneously distributedferromagnetic particles throughout the strip.

It is another advantage of the present invention to provide a method forproducing a metal or alloy strip suitable for use as a magnetic mediumor as an intermediate material for making equiaxed or accicular ironparticles.

It is a still further advantage of the present invention to provide amethod for producing a metal or alloy strip containing copper and ironwhich is relatively inexpensive to manufacture.

Accordingly, there has been provided a method for producing a stripuseful as a magnetic recording medium or an intermediate material formaking iron particles. A melt of molten metal or metal alloy containingabove about 20% by weight of iron is solidified so that equiaxed iron oriron alloy particles, between about 0.05 to about 0.5 microns indiameter, are distributed substantially homogeneously throughout thesolidified base metal matrix. The solidified mixture may be cold rolledinto a thin strip so that the iron particles together with the matrixelongate.

The invention and further developments of the invention are nowelucidated by means of preferred embodiments shown in the drawings:

FIG. 1 is a diagrammatical view of an apparatus for manufacturing a thinstrip of magnetic material in accordance with the present invention; and

FIG. 2 is a highly magnified view of a section of the manufacturedstrip.

The present invention relates to a method for producing a magneticrecording medium or intermediate material for making iron particles.First, a metal or alloy is melted by any conventional means. The basemetal preferably comprises copper or copper alloy. However, it is withinthe scope of the present invention to add other constituents such as thetransition metals described hereinbelow. Iron may be mixed into themolten base metal to form a substantially homogeneous single phase meltof the two metals. Although the iron may comprise above about 20% byweight of the entire mixture, the iron is preferably about 20 to about60% by weight of the mixture and most preferably between about 30 to 50%by weight of the mixture. The iron is preferably substantially purealthough it may contain some impurities or doping elements.

Although the invention is primarily described using only copper andiron, it is also within the scope of the present invention to add someother desired components to the melt to effect the operating parametersof the metallic strip if it is used as a magnetic recording medium.Transition metal additions that enhance the magnetic performance of theiron particles may be incorporated by alloying the melt. Nickel, cobalt,manganese and other transition elements in an effective amount up toweight percents of about 10% maximum and preferably between about 2 toabout 7% are advantageous for this purpose and are within the scope ofconventional alloying techniques. Other metal additions that primarilypartition to the copper or copper alloy to enhance the performance ofthe strip may also be incorporated into the melt.

The metal or alloy strip can be conveniently manufactured with anapparatus as shown in FIG. 1. There, an apparatus 10 is illustrated forproducing a continuous long thin strip 12 of copper or copper alloydispersed with iron. The mixture of molten copper base metal and iron 14may be introduced into a heat resisting tube 16 which may be composed ofquartz. The tube 16 is provided with a nozzle 18 having a diameter ofabout 0.3 to about 1.5 mm at one end. The molten material 14 ispreferably maintained at any desired temperature slightly above theliquidus point of the melt by any suitable means such as a heat resistor20. Notwithstanding the above temperature limitations, the moltenmaterial may be maintained at any desired temperature. Although thetemperature may be not more than about 200° C. above the liquidus, it ispreferably not more than about 100° C. above the liquidus. A coolingsubstrate 22, such as a chill wheel, is rotatably arranged below theheat resisting tube 16. The chill wheel may be of any desired diameterand may be rotated with a peripheral speed of between approximately1,050 to 8,400 feet per minute (fpm) and preferably between about 2,100to 4,200 fpm. However, it is within the scope of the present inventionto rotate the wheel at any desired speed. The open end 18 of the nozzleis preferably positioned less than about 5 mm and preferably less thanabout 2 mm from the smooth surface 24 of the wheel 22. The moltenmaterial is ejected from the tube 16 on to the rotating surface 24 undera pressure of between about 5 to about 40 psi and preferably betweenabout 15 to about 25 psi applied to the melt 14. As soon as the moltenmaterial contacts the rotating surface 24, the melt quickly cools andsolidifies into a thin continuous strip 12 having the iron or iron alloyparticles distributed substantially homogeneously or isotropicallythroughout the copper base metal matrix.

There are two precipitation modes of iron from a rapidly solidifiedcopper-iron melt. The primary solidification tends to be relativelycourse and plate like. These particles have a size greater thanapproximately 2μ. The secondary solidification which occurs at theterminal stage of solidification is much finer and more equiaxed. Thesubstantially equiaxed particles may be spherical or cubical inmorphology and have a size in the range of about 0.5μ to about 0.5μ. Theequiaxed particles make up the majority of the iron particles in theprimarily copper matrix.

The thickness and width of the obtained thin strip 12 can be determinedby a number of factors. For example, the surface tension between themolten material and the surface 24 of the moving chill wheel 22 affectsthe shape of strip 12. As the surface tension of the melt increasesrelative to the wheel, the strip tends to be thicker and narrower. Anincrease in the rotational speed of the chill wheel forms a thinner,wider strip. The ejection pressure of the melt 14 also acts to shape thestrip. As the pressure increases, the width of the strip increases whileits thickness decreases. The diameter of the nozzle being between about0.3 to about 1.5 mm and preferably between about 0.8 to about 1.2 mm isa factor. The smaller the diameter of the nozzle, the thinner and morenarrow the strip. Of course, the ejection temperature and viscosity ofthe melt are also critical factors. The hotter and less viscous themelt, the thinner and wider the strip. The viscosity is thought to be inthe range of about 0.01 to about 1 poise.

The selection of the material forming the chill wheel must take intoaccount the wettability between the molten thin strip and the surface24. This wettability is mainly determined by surface tensions of themelt and the substrate. It has been found that a chill wheel formed ofcopper can be successfully used to manufacture strip of the materialsset forth hereinabove. However, it is also within the terms of thepresent invention to use other materials such as for example, copperalloy, aluminum, aluminum alloy, steel, steel alloy or graphite.

The temperature of the molten material or melt is preferably slightlyabove its liquidus point. As mentioned above, although the temperaturemay be not more than about 200° C. above the liquidus point, it ispreferably not more than about 100° C. above the liquidus point. If thetemperature were below the liquidus point, the mixture would containsome solid particles and would not form properly. Conversely, if thetemperature were too high above the melting point, the melt might eitherspread over the cooling surface of the chill wheel so that the stripbecomes too thin or spray off the wheel before solidifying into a strip.Accordingly, the preferred temperature is slightly above the liquiduspoint so that the chill wheel can extract enough heat to immediatelymake the strip slightly solid and give it some mechanical stability orstrength. Depending upon the particular composition of the melt andother operating parameters of the process, the cooling rate might beabout 10² ° to 10⁸ ° K. per second and preferably between about 10² ° toabout 10⁶ ° K. per second.

Although a chill wheel is described as the preferred apparatus forforming the strip, it is also within the terms of the present inventionto form the strip by any desired conventional means.

The present invention is primarily concerned with the formation of stripthat is useful as a magnetic recording medium or as an intermediatematerial to produce iron or iron alloy particles. The process of formingthe strip is controlled so that the majority of these ferromagneticparticles are homogeneously distributed throughout the strip ofnon-magnetic metal matrix, equiaxed, i.e. spherical or cubical in shape,and preferably sized so that each particle is a single magnetic domain,i.e. in the range of about 0.05 to about 0.5 microns in thickness. Theparticle size is determined by solid solidification time which in turnis determined by factors such as the casting rate, thickness of thecasting and the thermal conductivity of the alloy. Thicker castingsections produce larger particles while thinner casting sections producesmaller particles. In general, a faster cooling rate results in theformation of smaller particles.

A typical example is a melt of molten copper containing about 30% byweight of iron. The molten stream is ejected onto the chill wheel by agas pressure of about 15 to 25 psi. The nozzle is located about 1 mmfrom the surface of the chill wheel. The chill wheel is made of copperand rotates at about 3,150 fpm. The resulting strip is about 2 to 3 mmin width and has a thickness of about 0.05 mm. The iron particles areisotropically or homogeneously dispersed throughout the copper matrixwith a majority being substantially equiaxed and having a diameter orthickness of about 0.1 micron or less.

The final copper or copper alloy strip, in accordance with the presentinvention, may provide acicular ferromagnetic particles, i.e. iron, bothisotropically or homogeneously dispersed throughout the matrix and witha high level or orientation in the longitudinal direction. So far, theprocess described has formed ferromagnetic particles being substantiallyequiaxed, i.e. spherical or cubical in shape and homogeneously orisotropically spaced throughout the matrix. The next step is directed toelongating the particles and orienting them in the longitudinaldirection. To accomplish this, the cast strip is preferably cold rolledto obtain the desired aspect ratio and orientation of the particles aswell as the final thickness of the strip. The aspect ratio of the newwrought particles, i.e. the ratio of the length to width, is preferablybetween about 5:1 and about 7:1 although it may be in the range of about4:1 to about 15:1. As the solidified melt is rolled into a thin strip,the iron or iron alloy particles 28, as shown in FIG. 2, elongate withtheir longitudinal dimension 29 in substantial alignment with thedirection of rolling or the longitudinal axis 30 extending through thestrip 12. The transverse section of smallest dimension of the wroughtferrous particles, between about 0.05 to about 0.5 microns, ispreferably substantially perpendicular to the axis 30.

Due to the step of cold rolling, the strip may be very stiff anddifficult to wrap around spools or to use as required. It, therefore,may be desirable to anneal the strip and soften it as required. Tosoften the wrought iron particles, the annealing would requiretemperatures in the range of about 400° to about 900° C. The strip canbe annealed in this range without changing particle morphology.

Once the strip with either the equiaxed or accicular particles isformed, it may be desirable to plate it with a protective material suchas a smooth electrode copper deposit. The plating preferaby has athickness of about 100 to about 500 microinches and preferably betweenabout 200 to about 300 microinches. The plating may be applied by anydesired technique such as conventional electrochemical plating.

The tape, whether plated or not, requires protection from tarnishing andcorrosion. This may be accomplished by passing the tape through staininhibitors such as benzotriazole or tolutriazole. These stain inhibitorsalso improve the lubricity of the strip to decrease the wear when usedagainst a device such as a tape head. Other materials which provide theproperties of tarnish and corrosion resistance as well as lubricityinclude copper fatty acid layers.

The patents set forth in this application are intended to beincorporated by reference herein.

It is apparent that there has been provided in accordance with thisinvention a method for producing a metal alloy strip havingsubstantially equiaxed or accicular iron or iron alloy particlesdistributed throughout which satisfies the objects, means, and advantgesset forth hereinabove. While the invention has been described incombination with the embodiments thereof, it is evident that manyalternatives, modifications, and variations will be apparent to thoseskilled in the art in light of the foregoing description. Accordingly,it is intended to embrace all such alternatives, modificatons, andvariations as fall within the spirit and broad scope of the appendedclaims.

We claim:
 1. A metallic strip consisting essentially of:about 20 toabout 60% by weight of iron and the balance being a material selectedfrom the group consisting of copper and alloys thereof, said materialforming a matrix; said metallic strip being characterized by having fineacicular particles of iron or iron alloy distributed substantiallyhomogeneously throughout said matrix, said acicular particles having awidth between about 0.05 to about 0.5 microns and an aspect ratio ofbetween about 4:1 to 15:1.
 2. The metallic strip of claim 1 furtherconsisting essentially of an effective amount for enhancing magneticperformance of up to about 10% by weight of a transition metal otherthan iron.
 3. The metallic strip of claim 2 wherein said transitionmetal is selected from the group consisting of nickel, cobalt, andmanaganese.
 4. The metallic strip of claim 1 wherein said acicularparticles have an aspect ratio of between about 5:1 to 7:1.
 5. Themetallic strip of claim 4 further comprising said strip having alongitudinal axis extending therethrough and said acicular particleshaving a longitudinal axis extending therethrough, said longitudinalaxis of said acicular particles being aligned with the longitudinal axisof said strip.
 6. The metallic strip of claim 5 further comprising saidstrip having been plated with a protective covering of copper.
 7. Themetallic strip of claim 6 further comprising a stain inhibitor coveringthe plated copper covering.
 8. A metallic strip consisting essentiallyof:about 20 to about 60% by weight of iron and the balance being amaterial selected from the group consisting of copper and alloysthereof, said material forming a matrix; said metallic strip beingcharacterized by having fine, substantially equiaxed particles of ironor iron alloy distributed substantially homogeneously throughout saidmatrix, said equiaxed particles having a width between about 0.05 toabout 0.5 microns.
 9. The metallic strip of claim 8 further consistingessentially of an effective amount for enhancing magnetic performance ofup to about 10% by weight of a transition metal other than iron.
 10. Themetallic strip of claim 9 further comprising said transition metal beingselected from the group consisting of nickel, cobalt, and manganese. 11.The metallic strip of claim 10 further comprising said strip beingplated with a protective covering of copper.
 12. The metallic strip ofclaim 11 further comprising a stain inhibitor covering the plated coppercovering.
 13. As an article of manufacture, a product formed by themethod of producing a metallic strip comprising the steps of:providing amelt of metal alloy consisting essentially of about 20 to about 60% byweight of iron and the balance being a material selected from the groupconsisting of copper and alloys thereof, said material forming a matrix;and rapidly solidifying said melt into said metallic strip havingsustantially fine, equiaxed particles of iron or iron alloy distributedsubstantially homogeneously throughout said matrix said equiaxedparticles having a width between about 0.05 to about 0.5 microns. 14.The article of manufacture of claim 13 further including the step ofadding to said melt an effective amount for enhancing magneticperformance of up to about 10% by weight of a transition metal or otherthan iron.
 15. The article of manufacture of claim 14 including the stepof rolling said strip to elongate the iron or iron alloy particles.